A new nickel(II)-dicyanamide compound, [Ni(dca)2(en)]n (1) (dca=dicyanamide anion, -); en=ethylene diamine), has been synthesized and its structure has been determined by single crystal X-ray diffraction analysis. The...A new nickel(II)-dicyanamide compound, [Ni(dca)2(en)]n (1) (dca=dicyanamide anion, -); en=ethylene diamine), has been synthesized and its structure has been determined by single crystal X-ray diffraction analysis. The crystal is monoclinic, space group P21/n with unit cell dimensions: a=0.694 3(1) nm, b=1.041 5(2) nm, c=1.413 2(2) nm, and β=90.381°, Z=4, V=1.011 0(3) nm3. In this compound, the adjacent nickel atoms are connected by dca all inμ1,5-bridging mode to form ladder-like units, which are linked with double dca bridges to generate a regular infinite stair-like structure. Temperature-dependent magnetic susceptibility was also characterized for this compound. CCDC: 208276.展开更多
The title complex {[AgL]ClO4}n（L=2,5-bis（3-pyridinylmethylthio）-1,3,4-thiadiazole） was synthesized by the reaction of Ag（I） salt and a novel flexible ligand L.Its structure was determined by X-ray crystallograph...The title complex {[AgL]ClO4}n（L=2,5-bis（3-pyridinylmethylthio）-1,3,4-thiadiazole） was synthesized by the reaction of Ag（I） salt and a novel flexible ligand L.Its structure was determined by X-ray crystallography with the following data：monoclinic,space group P21/n,a=16.5068（13）,b=7.6548（4）,c=16.5521（13）A,β=115.119（3）o,V=1893.7（2）A^3,Z=4,Dc=1.893 g/cm^3,μ=1.565 mm^-1,F（000）=1072,C14H12AgClN4O4S3,Mr=539.78,T=293（2） K,S=1.067,the final R=0.0342 and wR=0.0870.The silver ion in the complex is in a trigonal coordination geometry to link three different L.Meanwhile,each L connects three different silver ions by its N coordination sites to form a two-dimensional layer structure.展开更多
Two comparable discrete complexes [CuⅡ（CH3CN）2L2]·2（ClO4） 1 and [CuI2I2L2]·（DMF）2 2 were successfully synthesized by the reaction of CuⅡ and CuⅠ salts with a novel dinucleating ligand 2,5-bis（3-pyr...Two comparable discrete complexes [CuⅡ（CH3CN）2L2]·2（ClO4） 1 and [CuI2I2L2]·（DMF）2 2 were successfully synthesized by the reaction of CuⅡ and CuⅠ salts with a novel dinucleating ligand 2,5-bis（3-pyridinylmethylthio）-1,3,4-thiadiazole）（L）,respectively.Complex 1 presents a single nuclear structure while 2 has a dimeric structure where two CuI ions are doubly bridged by halide ions in a μ2-fashion.Both discrete molecules were outspreaded into a one-dimensional supramolecular chain via aromatic interactions such as C–H…π and π…π interactions.展开更多
The reaction of lanthanum（Ⅲ） nitrate and 5-nitroisophthalic acid in isopropanol/H2O under hydrothermal conditions leads to a 3D lanthanum-containing coordination polymer with the general chemical formula {[La6（Nip...The reaction of lanthanum（Ⅲ） nitrate and 5-nitroisophthalic acid in isopropanol/H2O under hydrothermal conditions leads to a 3D lanthanum-containing coordination polymer with the general chemical formula {[La6（Nip）9（H2O）4 ]·（H2O）4 }∞（1,Nip=5-nitroisophthalate）.The single-crystal X-ray analyses show that this compound crystallizes in the orthorhombic system,space group Ima2 with a=9.7769（12）,b=28.239（3）,c=21.149（2）,V=5839.1（11）3,Z=2,Mr=2859.61,Dc =1.626 g/cm 3,F（000）=2752.14040 reflections are collected,of which 5275 are unique （R int=0.0241）.Final GOOF=1.083,R=0.0406 and wR=0.1182,R indices based on 5183 reflections with I〉2σ（I）（refinement on F2）,443 parameters,1 restraint.Lp and absorption corrections were applied,=2.242mm-1.Absolute structure parameter x=0.08（3）.The crystal structure can be described as the butterfly-liked hexanuclear lanthanum entities {La6O6（CO2）8 } covalently linked to each other by nitroisophthalate ligands into an intricate three-dimensional structure.The fluorescence spectroscopy of compound 1 has been investigated.展开更多
A metal-organic coordination polymer [Co(ip)(phen)]n (ip = isophthalate, phen = 1,10-phenanthroline) 1 has been hydrothermally synthesized and characterized. Compound 1 crystallizes in P2/c space group with a = 8.37(2...A metal-organic coordination polymer [Co(ip)(phen)]n (ip = isophthalate, phen = 1,10-phenanthroline) 1 has been hydrothermally synthesized and characterized. Compound 1 crystallizes in P2/c space group with a = 8.37(2), b = 10.41(1), c = 18.36(3) ?, β = 100.41(7)o, C20H12CoN2O4, Mr = 403.25, V = 1573(4) ?3, Z = 4 and Dc = 1.703 g/cm3. Two Co(II) ions are bridged by μ-carboxylate to form a dinuclear unit, which is extended by ip ligands resulting in a ribbon-like chain. Pairs of phen ligands attach to the dinuclear units on both sides of the chain alternately. Magnetic study reveals that the interaction between the carboxylate-bridged Co(II) ions in 1 is weakly antiferromagnetic.展开更多
A three-dimensional complex [Cu（3-ampy）（HEO）4]（SO4）·（H2O） （3-ampy = 3-amino- pyridine） has been synthesized. Crystallographic data： C5H16CuN2O9S, Mr = 343.80, triclinic, space group P1, a = 7.675（2）,...A three-dimensional complex [Cu（3-ampy）（HEO）4]（SO4）·（H2O） （3-ampy = 3-amino- pyridine） has been synthesized. Crystallographic data： C5H16CuN2O9S, Mr = 343.80, triclinic, space group P1, a = 7.675（2）, b = 8.225（3）, c = 10.845（3）A, α= 86.996（4）, β = 76.292（4）, γ= 68.890（4）°, V = 620.0（3）A^3, Z = 2, Dc = 1.841 g/cm^3, F（000） = 354 and μ = 1.971 mm^-1. The structure was refined to R = 0.0269 and wR = 0.0659 for 1838 observed reflections （I 〉 2a（/））. The structure consists of [Cu（3-ampy）（H2O）4]^2＋ cations, SO4^2- anions and lattice water molecules. 3-Ampy acting as a bidentate bridging ligand generates a 1D covalent chain. A supramolecular 2D framework is formed through π-π stacking of pyridine rings. The lattice water molecules and SO4^2- anions are located between the adjacent 2D frameworks. The hydrogen bonding interactions from lattice water molecules and SO4^2- anions to coordinate water extend the 2D framework into a 3D network.展开更多
The title complex, [ [ Cd（Him） （OH-BDC） （H2O）2 ]· 3H2O]n （ 1 ） （Him is imidazole, OH-H2BDC is 5-hydroxyisophthalic acid）, was synthesized by liquid/liquid diffusion method at room temperature. The compl...The title complex, [ [ Cd（Him） （OH-BDC） （H2O）2 ]· 3H2O]n （ 1 ） （Him is imidazole, OH-H2BDC is 5-hydroxyisophthalic acid）, was synthesized by liquid/liquid diffusion method at room temperature. The complex crystallizes in orthorhombic, space group P212121, with a = 0.671 6 （7）, b = 1.380 6 （2）, c = 1.7421（2） nm, V = 1.615 2（3） nm3, C11H18CdN2O10, Mr = 450.67, Dc = 1.853 g/cm3, μ = 1.407 mm^-1, F（000） = 904, Z = 4, the final R1 = 0.020 9 and wR2 = 0.045 3 for 3 211 observed reflections （Ⅰ 〉 2σ （Ⅰ））. In the structure of 1, the OH-BDC ligands exhibiting bis-bidentate coordination mode bridge the adjacent Cd centers to form a one-dimensional helical chain and the second ligand Him acting as terminal ligands are attached to the helical chain. It is notable that a series of complicated hydrogen bonds （e. g., N-H… O, O-H… O） exist in the structure, which link neighboring helices into a three-dimensional supramolecular architeeture. An observed intense blue luminescence with an emission band peaking at 390 nm for 1 may be resulted from ligand-to-metal charge transfer （LMCT）.展开更多
6-（3,5-Dimethylpyrazol-1-yl）-3-（2,4,6-trinitroanilino）-1,2,4,5-tetrazin （1） has been synthesized and characterized by ^1H NMR, MS, elemental analysis, infrared spectra and thermal analyses. The crystal structure...6-（3,5-Dimethylpyrazol-1-yl）-3-（2,4,6-trinitroanilino）-1,2,4,5-tetrazin （1） has been synthesized and characterized by ^1H NMR, MS, elemental analysis, infrared spectra and thermal analyses. The crystal structure was determined by X-ray diffraction method. 1 is crystallized in P21/c space group of monoclinic crystal system, and exhibits good physical properties, such as high densities （〉 1.55 g·cm^-3） and good thermal stabilities （Td〉220 ℃）. The intrermolecular hydrogen bonds construct the P- and M-helices from organic molecules and may contribute to the high melting points.展开更多
文摘A new nickel(II)-dicyanamide compound, [Ni(dca)2(en)]n (1) (dca=dicyanamide anion, -); en=ethylene diamine), has been synthesized and its structure has been determined by single crystal X-ray diffraction analysis. The crystal is monoclinic, space group P21/n with unit cell dimensions: a=0.694 3(1) nm, b=1.041 5(2) nm, c=1.413 2(2) nm, and β=90.381°, Z=4, V=1.011 0(3) nm3. In this compound, the adjacent nickel atoms are connected by dca all inμ1,5-bridging mode to form ladder-like units, which are linked with double dca bridges to generate a regular infinite stair-like structure. Temperature-dependent magnetic susceptibility was also characterized for this compound. CCDC: 208276.
基金Supported by the National Natural Science Foundation of China (Nos 20801004/B01, 20871016/B0101, 10876002/A06)the 111 Project (B07012)Excellent Young Scholars Research Fund of Beijing Institute of Technology (No 2006Y0715)
文摘The title complex {[AgL]ClO4}n（L=2,5-bis（3-pyridinylmethylthio）-1,3,4-thiadiazole） was synthesized by the reaction of Ag（I） salt and a novel flexible ligand L.Its structure was determined by X-ray crystallography with the following data：monoclinic,space group P21/n,a=16.5068（13）,b=7.6548（4）,c=16.5521（13）A,β=115.119（3）o,V=1893.7（2）A^3,Z=4,Dc=1.893 g/cm^3,μ=1.565 mm^-1,F（000）=1072,C14H12AgClN4O4S3,Mr=539.78,T=293（2） K,S=1.067,the final R=0.0342 and wR=0.0870.The silver ion in the complex is in a trigonal coordination geometry to link three different L.Meanwhile,each L connects three different silver ions by its N coordination sites to form a two-dimensional layer structure.
基金Supported by the National Natural Science Foundation of China (Nos 20801004/B01, 20871016/B0101, 10876002/A06)the 111 Project (B07012)Excellent Young Scholars Research Fund of Beijing Institute of Technology (No 2006Y0715)
文摘Two comparable discrete complexes [CuⅡ（CH3CN）2L2]·2（ClO4） 1 and [CuI2I2L2]·（DMF）2 2 were successfully synthesized by the reaction of CuⅡ and CuⅠ salts with a novel dinucleating ligand 2,5-bis（3-pyridinylmethylthio）-1,3,4-thiadiazole）（L）,respectively.Complex 1 presents a single nuclear structure while 2 has a dimeric structure where two CuI ions are doubly bridged by halide ions in a μ2-fashion.Both discrete molecules were outspreaded into a one-dimensional supramolecular chain via aromatic interactions such as C–H…π and π…π interactions.
基金financially supported by the National Natural Science Foundation of China (20731002,10876002,and 21173021)the 111 Project(B07012)+2 种基金the Program of Cooperation of the Beijing Education Commission (20091739006)Specialized Research Fund for the Doctoral Program of Higher Education (200800070015)Beijing Municipal Science & Technology Commission (Z09010300820902)
文摘The reaction of lanthanum（Ⅲ） nitrate and 5-nitroisophthalic acid in isopropanol/H2O under hydrothermal conditions leads to a 3D lanthanum-containing coordination polymer with the general chemical formula {[La6（Nip）9（H2O）4 ]·（H2O）4 }∞（1,Nip=5-nitroisophthalate）.The single-crystal X-ray analyses show that this compound crystallizes in the orthorhombic system,space group Ima2 with a=9.7769（12）,b=28.239（3）,c=21.149（2）,V=5839.1（11）3,Z=2,Mr=2859.61,Dc =1.626 g/cm 3,F（000）=2752.14040 reflections are collected,of which 5275 are unique （R int=0.0241）.Final GOOF=1.083,R=0.0406 and wR=0.1182,R indices based on 5183 reflections with I〉2σ（I）（refinement on F2）,443 parameters,1 restraint.Lp and absorption corrections were applied,=2.242mm-1.Absolute structure parameter x=0.08（3）.The crystal structure can be described as the butterfly-liked hexanuclear lanthanum entities {La6O6（CO2）8 } covalently linked to each other by nitroisophthalate ligands into an intricate three-dimensional structure.The fluorescence spectroscopy of compound 1 has been investigated.
基金This work was supported by the NNSFC, NSF and Young Scientist Foundation of Fujian Province
文摘A metal-organic coordination polymer [Co(ip)(phen)]n (ip = isophthalate, phen = 1,10-phenanthroline) 1 has been hydrothermally synthesized and characterized. Compound 1 crystallizes in P2/c space group with a = 8.37(2), b = 10.41(1), c = 18.36(3) ?, β = 100.41(7)o, C20H12CoN2O4, Mr = 403.25, V = 1573(4) ?3, Z = 4 and Dc = 1.703 g/cm3. Two Co(II) ions are bridged by μ-carboxylate to form a dinuclear unit, which is extended by ip ligands resulting in a ribbon-like chain. Pairs of phen ligands attach to the dinuclear units on both sides of the chain alternately. Magnetic study reveals that the interaction between the carboxylate-bridged Co(II) ions in 1 is weakly antiferromagnetic.
基金the Natural Science Found Council of China (Nos. 20671011, 20331010, 90406002 and 90406024) the Key Laboratory of Structural Chemistry Foundation (No. 060017)
文摘A three-dimensional complex [Cu（3-ampy）（HEO）4]（SO4）·（H2O） （3-ampy = 3-amino- pyridine） has been synthesized. Crystallographic data： C5H16CuN2O9S, Mr = 343.80, triclinic, space group P1, a = 7.675（2）, b = 8.225（3）, c = 10.845（3）A, α= 86.996（4）, β = 76.292（4）, γ= 68.890（4）°, V = 620.0（3）A^3, Z = 2, Dc = 1.841 g/cm^3, F（000） = 354 and μ = 1.971 mm^-1. The structure was refined to R = 0.0269 and wR = 0.0659 for 1838 observed reflections （I 〉 2a（/））. The structure consists of [Cu（3-ampy）（H2O）4]^2＋ cations, SO4^2- anions and lattice water molecules. 3-Ampy acting as a bidentate bridging ligand generates a 1D covalent chain. A supramolecular 2D framework is formed through π-π stacking of pyridine rings. The lattice water molecules and SO4^2- anions are located between the adjacent 2D frameworks. The hydrogen bonding interactions from lattice water molecules and SO4^2- anions to coordinate water extend the 2D framework into a 3D network.
基金Sponsored by the National Natural Science Foundation of China (20371007 ,20476011 ,20771013)Excellent Young Scholars Research Fund of Beijing Institute of Technology(2006Y0715)
文摘The title complex, [ [ Cd（Him） （OH-BDC） （H2O）2 ]· 3H2O]n （ 1 ） （Him is imidazole, OH-H2BDC is 5-hydroxyisophthalic acid）, was synthesized by liquid/liquid diffusion method at room temperature. The complex crystallizes in orthorhombic, space group P212121, with a = 0.671 6 （7）, b = 1.380 6 （2）, c = 1.7421（2） nm, V = 1.615 2（3） nm3, C11H18CdN2O10, Mr = 450.67, Dc = 1.853 g/cm3, μ = 1.407 mm^-1, F（000） = 904, Z = 4, the final R1 = 0.020 9 and wR2 = 0.045 3 for 3 211 observed reflections （Ⅰ 〉 2σ （Ⅰ））. In the structure of 1, the OH-BDC ligands exhibiting bis-bidentate coordination mode bridge the adjacent Cd centers to form a one-dimensional helical chain and the second ligand Him acting as terminal ligands are attached to the helical chain. It is notable that a series of complicated hydrogen bonds （e. g., N-H… O, O-H… O） exist in the structure, which link neighboring helices into a three-dimensional supramolecular architeeture. An observed intense blue luminescence with an emission band peaking at 390 nm for 1 may be resulted from ligand-to-metal charge transfer （LMCT）.
文摘6-（3,5-Dimethylpyrazol-1-yl）-3-（2,4,6-trinitroanilino）-1,2,4,5-tetrazin （1） has been synthesized and characterized by ^1H NMR, MS, elemental analysis, infrared spectra and thermal analyses. The crystal structure was determined by X-ray diffraction method. 1 is crystallized in P21/c space group of monoclinic crystal system, and exhibits good physical properties, such as high densities （〉 1.55 g·cm^-3） and good thermal stabilities （Td〉220 ℃）. The intrermolecular hydrogen bonds construct the P- and M-helices from organic molecules and may contribute to the high melting points.
